Reaktion #91480

ord-6548f0433bdd4c3c9ebe2ed0cfadbf32

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe precipitate was removed by filtration, and MeOH
  2. 2
    Sonstigewas removed
  3. 3
    Sonstigeevaporation
  4. 4
    workup.ADDITIONTo the remaining solution was added 1M HCl
  5. 5
    Sonstigeto adjust to pH=2 under 0° C
  6. 6
    FiltrationThe resulting precipitate was filtered

Vorschrift

Benzonitrile (40 mmol) was combined with L-cysteine (45 mmol) in 100 mL of 1:1 MeOH/pH 6.4 phosphate buffer solution. The reaction was stirred at 40° C. for 3 days. The precipitate was removed by filtration, and MeOH was removed using rotary evaporation. To the remaining solution was added 1M HCl to adjust to pH=2 under 0° C. The resulting precipitate was filtered to yield a white solid 2-phenyl-4,5-dihydrothiazole-4-carboxylic acid 42a, which was used directly to next step without purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447049B2uspto-grants-2016_09